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WO2017090498A1 - Procédé de production de film de barrière contre les gaz - Google Patents

Procédé de production de film de barrière contre les gaz Download PDF

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Publication number
WO2017090498A1
WO2017090498A1 PCT/JP2016/083998 JP2016083998W WO2017090498A1 WO 2017090498 A1 WO2017090498 A1 WO 2017090498A1 JP 2016083998 W JP2016083998 W JP 2016083998W WO 2017090498 A1 WO2017090498 A1 WO 2017090498A1
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WO
WIPO (PCT)
Prior art keywords
layer
transition metal
gas barrier
film
vapor deposition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2016/083998
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English (en)
Japanese (ja)
Inventor
健治 属
河村　朋紀
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Konica Minolta Inc
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Konica Minolta Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Konica Minolta Inc filed Critical Konica Minolta Inc
Priority to JP2017552375A priority Critical patent/JPWO2017090498A1/ja
Publication of WO2017090498A1 publication Critical patent/WO2017090498A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering

Definitions

  • FIG. 1 is a sputtering apparatus
  • 2 is a vacuum chamber
  • 3 is a supply-side transfer system chamber
  • 4 is a storage-side transfer system chamber
  • 5 is a delivery roller
  • 6, 7, 8, 9 are transfer rollers
  • 10 is a winding roller.
  • 30 is a gas barrier film
  • 31 is a substrate
  • 32 is a first layer containing a non-transition metal (M1)
  • 32a is a region other than the composite composition region
  • 32b is a composite composition region (oxygen deficient region).
  • 33 represents a second layer containing a transition metal (M2)
  • 34 represents a third layer containing a transition metal (M2).
  • a composite composition region containing the non-transition metal (M1) and the transition metal (M2) is formed in the vicinity of the interface between the layer containing the non-transition metal (M1) and the layer containing the transition metal (M2).
  • the composite composition region has an oxygen deficient composition, and it is difficult for the non-transition metal (M1) and the transition metal (M2) to form a bond only with oxygen. Become.
  • a non-transition metal (M1) simple substance or a compound containing a non-transition metal (M1) may be used as a raw material for forming the first layer.
  • the compound containing the non-transition metal (M1) is not particularly limited, and examples thereof include organometallic compounds, oxides, nitrides, oxynitrides, oxycarbides, and the like.
  • the suitable example of the compound containing a non-transition metal (M1) in case a non-transition metal (M1) is Si is mentioned later.
  • the compound containing the non-transition metal (M1) is polysilazane
  • the composition of the gas barrier layer finally obtained by storage over time until the second layer is formed can be suppressed, and productivity and production can be suppressed. This is because the stability is improved.
  • a sol-gel method may be used as the coating method for forming the first layer as described in JP-A-2005-231039.
  • the coating liquid used when forming the modified layer by the sol-gel method preferably contains alkoxysilane and at least one of a polyvinyl alcohol resin and an ethylene / vinyl alcohol copolymer. Further, the coating liquid preferably contains a sol-gel method catalyst, an acid, water, and an organic solvent. In the sol-gel method, a modified layer is obtained by polycondensation using such a coating solution.
  • R 1 , R 2 and R 3 are each independently a hydrogen atom, a substituted or unsubstituted alkyl group, aryl group, vinyl group or (trialkoxysilyl) alkyl group. . At this time, R 1 , R 2 and R 3 may be the same or different.
  • Perhydropolysilazane is presumed to have a linear structure and a ring structure centered on 6- and 8-membered rings.
  • the number average molecular weight (Mn) is about 600 to 2000 (polystyrene conversion), and there are liquid or solid substances, and the state varies depending on the molecular weight.
  • the solvent for preparing the coating liquid for forming the first layer is not particularly limited as long as it can dissolve the compound containing the non-transition metal (M1).
  • M1 the compound containing the non-transition metal
  • it does not contain water and reactive groups (for example, hydroxyl group or amine group) that easily react with polysilazane, and does not contain polysilazane.
  • Inert organic solvents are preferred, and aprotic organic solvents are more preferred.
  • the coating solution preferably contains a catalyst from the viewpoint of accelerating reforming when reforming by vacuum ultraviolet rays.
  • the catalyst applicable to the present invention is preferably a basic catalyst, and in particular, an amine catalyst, a metal catalyst such as a Pt compound, a Pd compound, and an Rh compound, and an N-heterocyclic compound are exemplified. Of these, it is preferable to use an amine catalyst.
  • the amine catalyst is not particularly limited, and for example, N, N, N ′, N′-tetramethyl-1,6-diaminohexane or the like can be used.
  • the first layer After forming the first layer, it has a step of storing in a high-temperature and high-humidity environment by performing vacuum ultraviolet irradiation until the second layer is formed after forming the first layer. Even if it has, the composition of the gas barrier layer finally obtained hardly changes compared with the manufacturing method which does not have the process to preserve
  • the distance between the irradiation surface and the light source is preferably 0.5 to 10 mm.
  • the distance between the irradiation surface and the light source is 0.5 mm or more, scratches caused by contact between the substrate surface and the light source can be further reduced when the substrate is continuously processed while being conveyed.
  • the distance between the irradiation surface and the light source is 10 mm or less, it is possible to further suppress a decrease in the amount of light due to the vacuum ultraviolet absorbing gas existing between the substrate surface and the light source.
  • the vacuum ultraviolet ray used may be generated by plasma formed of a gas containing at least one of CO, CO 2 and CH 4 .
  • the gas containing at least one of CO, CO 2 and CH 4 hereinafter also referred to as carbon-containing gas
  • the carbon-containing gas may be used alone, but carbon containing rare gas or H 2 as the main gas. It is preferable to add a small amount of the contained gas. Examples of plasma generation methods include capacitively coupled plasma.
  • the raw material for forming the second layer or the third layer does not contain a non-transition metal (M1) or a compound containing a non-transition metal (M1). .
  • the second layer and the third layer are formed by a physical vapor deposition method (PVD method).
  • the physical vapor deposition (Physical Vapor Deposition) is a method of depositing a thin film of a target substance on the surface of the substance in a gas phase by a physical method.
  • the physical vapor deposition method can be roughly divided into an evaporation system and a sputtering system.
  • the transition metal (M2) simple substance or transition metal (M2) oxide film, nitride film, oxynitride film, or oxycarbide film is formed by sputtering using bipolar sputtering, magnetron sputtering, or an intermediate frequency region.
  • T2 (nm) and T3 (nm) are obtained by performing film formation using a base material in which vapor deposition particles do not easily enter the interior in advance under the film formation conditions of the second layer and the third layer. It can be obtained by measuring the thickness of the obtained layer and dividing the thickness by the deposition time.
  • the glass base material is used as a base material for a measurement.
  • a commercially available glass substrate can be used, and for example, Corning's Willow Glass can be used.
  • T2 (nm) is not particularly limited, but is preferably 0.5 nm or more, and more preferably 0.5 nm or more and 5.0 nm or less.
  • the thickness is 0.5 nm or more, a further gas barrier property improving effect and a further low haze reducing effect can be obtained. This is presumably because the distance that the vapor deposition particles enter the layer containing the non-transition metal (M1) becomes larger, and a uniform composite composition region can be formed with a larger film thickness.
  • the further improvement effect of gas barrier property and the further haze reduction effect can be acquired as it is 5.0 nm or less.
  • the method for producing a gas barrier film according to an embodiment of the present invention includes steps 2 and 3,
  • the deposition time for forming the second layer is t2 (seconds) and the deposition time t3 (seconds) for forming the third layer is t2 (seconds) and t3 (seconds)
  • the equipment and structure of the region for forming the second layer is the same as the equipment and structure of the region for forming the third layer in the roll-to-roll method.
  • a method using a certain apparatus is mentioned. This is because when the base material is transported at a constant transport speed in such an apparatus, the time required for the deposition base material to pass through the region for forming the second layer, and the deposition base material for the third layer. This is because the time for passing through the region for formation is the same.
  • the second layer and the third layer are formed of the reaction gas type, the target type, the pressure, the transport speed of the film (deposition substrate), the diameter of the film forming roller provided in the apparatus, and the evaporation source and the evaporation surface. It can be manufactured as a layer having desired characteristics by appropriately adjusting the opening length in the conveying direction regulated by the adhesion-preventing plate installed therebetween.
  • the power source used for the sputtering method is not particularly limited, but a DC power source, a DC pulse power source, or an MF power source is preferably used from the viewpoint of the deposition rate.
  • a DC power source for example, DC power supplies DPG-10, DPG-10H, DPG-20 and DPG-20H manufactured by ULVAC, Inc., DC pulse power supply of Advanced Energy, Inc., Pinplus Plus + (trademark) 5K, 10K, 5K Dual, TF power source MF Generators TruPlasma MF Series 7000 etc. can be used.
  • the content of the reactive gas in the sputtering gas in the reactive sputtering method is not particularly limited, but the partial pressure of the reactive gas is preferably 1 to 50% with respect to the total pressure of the sputtering gas, and is preferably 3 to 30%. More preferably, it is more preferably 5 to 20%.
  • the supply-side transfer system chamber 3 and the storage-side transfer system chamber 4 are each connected to a vacuum pump 18, and the pressure in the supply-side transfer system chamber 3 and the storage-side transfer system chamber 4 is changed by the vacuum pump, respectively. It is possible to adjust appropriately independently.
  • the sputtering apparatus 1 includes a load lock 21 between the vacuum chamber 2 and the supply-side transfer system chamber 3, and includes a load lock 22 between the vacuum chamber 2 and the storage-side transfer system chamber 4. ing. With the load locks 21 and 22, even if the supply-side transport system chamber 3 and the storage-side transport system chamber 4 are opened to the atmosphere by roll exchange or the like, the vacuum state in the vacuum chamber 2 can be maintained while the film is passed. Can be held.
  • the second layer and the third layer are formed using at least two of the six cathodes.
  • the positions of the two cathodes for forming the second layer and the third layer are not particularly limited, but it is preferable to select two cathodes arranged adjacent to each other.
  • the remaining cathode can be used when further layers are formed. When seven or more layers are formed, for example, a structure in which two vacuum chambers 2 are coupled in series may be employed.
  • each chamber is arbitrarily airtightly maintained so that the pressures in the vacuum chamber 2, the supply-side transfer system chamber 3, and the storage-side transfer system chamber 4 can be appropriately adjusted independently. Anything that can do.
  • the load lock 21 and the load lock 22 are not particularly limited, and known load locks can be used as appropriate.
  • Known load locks include, for example, a load lock valve having two roller gates facing the inside, such as the apparatus shown in FIG. 1 of JP-A-2015-074810, or a film other than a roller gate. And a load lock valve provided with a flexible member having a shape that can be kept airtight.
  • each of the above-mentioned transition metal (M2) simple substance or A compound containing a transition metal (M2) can be used.
  • a manufacturing method is a method of manufacturing a laminate including both surfaces of a substrate, the surface of a substrate on the side on which the first layer is formed, or the first layer, the second layer, and the third layer. You may further have the process of forming a hard-coat layer in the outermost surface.
  • the material included in the hard coat layer is not particularly limited, and a known hard coat layer forming material can be used. Examples of the hard coat layer forming material include a thermosetting resin and an active energy ray curable resin, and an active energy ray curable resin is preferable because it can be easily molded. Such curable resins can be used singly or in combination of two or more.
  • the hard coat layer may be any layer that can impart hard coat properties, and may be a layer that also has other functions.
  • the heart coat layer may have an anti-block function, a function as the anchor coat layer described above, and a function as a smoothing layer described later.
  • a hard coat layer is a thing which has a function as an anchor coat layer, as a material contained in a hard coat layer, what can provide hard coat property among the above-mentioned anchor coat agents is preferably used. Can do.
  • the material included in the hard coat layer is preferably a material capable of imparting hard coat properties among the smooth layer forming materials described later. Can do.
  • the formation method of the hard coat layer is not particularly limited, but it is preferably formed by a wet coating method such as a spin coating method, a spray method, a blade coating method, a dip method, or a dry coating method such as an evaporation method.
  • a wet coating method in which a hard coat layer is formed using a hard coat layer forming solution is more preferable.
  • the manufacturing method which concerns on one form of this invention may further have the process of forming a smooth layer between a base material and a 1st layer.
  • the smooth layer used in the present invention flattens the rough surface of the resin base material where protrusions and the like exist, or flattens the unevenness and pinholes generated in the transparent inorganic compound layer by the protrusions existing on the resin base material.
  • Such a smooth layer is basically produced by curing a photosensitive material or a thermosetting material.
  • additives such as an antioxidant, an ultraviolet absorber, and a plasticizer can be added to the above-described photosensitive resin or thermosetting material as necessary.
  • an appropriate resin or additive may be used for improving the film formability and preventing the generation of pinholes in the film.
  • a clear hard coat layer having a thickness of 0.5 ⁇ m and having an antiblock function was formed on the surface of the substrate opposite to the surface on which the gas barrier layer was formed.
  • the clear hard coat layer is formed by applying a UV curable resin (manufactured by Aika Kogyo Co., Ltd., product number: Z731L) on the base material so that the dry film thickness is 0.5 ⁇ m, and then drying at 80 ° C. Thereafter, curing was performed under a condition of irradiation energy of 0.5 J / cm 2 using a high-pressure mercury lamp in the air.
  • a gas barrier film 2 was produced in the same manner as in the production of the gas barrier film 1 except that the sputtering power source power at the time of forming the second layer was 2.1 W / cm 2 .
  • gas barrier film 6 In the production of the gas barrier film 1, the gas barrier film 6 was produced in the same manner except that the sputtering power source power during the formation of the second layer was set to 5.2 W / cm 2 .
  • gas barrier film 7 In the production of the gas barrier film 1, the gas barrier film 7 was produced in the same manner except that the sputtering power source power at the time of forming the second layer was 5.6 W / cm 2 .
  • Haze is less than 0.5% 4: Haze is 0.5% or more and less than 1% 3: Haze is 1% or more and less than 1.5% 2: Haze is 1.5% or more and less than 2% 1: Haze is 2% or more
  • the gas barrier films 2 to 8 produced by the production methods according to the examples had high gas barrier properties and low haze.
  • the gas barrier film 9 according to the comparative example and the gas barrier film 10 according to the comparative example are the total film thicknesses of the second layer and the third layer than the gas barrier films 2 to 8 according to the example.
  • the gas barrier properties were inferior.
  • the further effect of improving the gas barrier property according to the present invention is not obtained due to the increase in the thickness of the layer containing the transition metal (M2), but the method for forming the layer containing the transition metal (M2). It was confirmed that it was obtained due to

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Physical Vapour Deposition (AREA)
  • Laminated Bodies (AREA)

Abstract

La présente invention concerne un procédé de production de film de barrière contre les gaz, ledit procédé comprenant : une étape 1 dans laquelle une première couche contenant un métal non-transition (M1) est formée sur un substrat en utilisant le métal non-transition (M1) ou un composé contenant le métal non-transition (M1) ; une étape 2 dans laquelle une deuxième couche contenant un métal de transition (M2) est formée sur la première couche, de manière à être en contact avec la première couche, en utilisant le métal de transition (M2) ou un composé contenant le métal de transition (M2) au moyen d'un dépôt physique en phase vapeur ; et une étape 3 dans laquelle une troisième couche contenant le métal de transition (M2) est formée sur la deuxième couche, de manière à être en contact avec la deuxième couche, en utilisant le métal de transition (M2) ou un composé contenant le métal de transition (M2) au moyen d'un dépôt physique en phase vapeur. Dans l'étape 2 et l'étape 3, si le taux de dépôt auquel la deuxième couche est formée est désigné par DR2 (nm/seconde) et le taux de dépôt auquel la troisième couche est formé est désigné par DR3 (nm/seconde), le rapport R de DR2 (nm/seconde) à DR3 (nm/seconde) satisfait à la formule 1. Formule 1 : 0,2 ≤ R < 0,9
PCT/JP2016/083998 2015-11-24 2016-11-16 Procédé de production de film de barrière contre les gaz Ceased WO2017090498A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2017552375A JPWO2017090498A1 (ja) 2015-11-24 2016-11-16 ガスバリア性フィルムの製造方法

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JP2015228884 2015-11-24
JP2015-228884 2015-11-24

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113441377A (zh) * 2021-06-29 2021-09-28 辽宁分子流科技有限公司 一种纳米银丝电极薄膜的制备方法

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH111769A (ja) * 1997-06-10 1999-01-06 Canon Inc スパッタ膜の製造方法及びスパッタ膜
JP2003202405A (ja) * 2002-01-08 2003-07-18 Matsushita Electric Ind Co Ltd 反射防止膜を有する光学素子およびその製造方法
JP2008231532A (ja) * 2007-03-22 2008-10-02 Mitsubishi Materials Corp 被銅メッキ処理材の製造方法
JP2009196155A (ja) * 2008-02-20 2009-09-03 Dainippon Printing Co Ltd ガスバリアフィルム、ガスバリア膜の作製方法及び作製装置
JP2009220342A (ja) * 2008-03-14 2009-10-01 Oike Ind Co Ltd ガスバリアフィルムの製造方法及びガスバリアフィルム
WO2011077738A1 (fr) * 2009-12-25 2011-06-30 株式会社アルバック Film décoratif pour le moulage d'inserts, article formé par moulage d'inserts, procédé pour produire un film décoratif pour moulage d'inserts
JP2012061683A (ja) * 2010-09-15 2012-03-29 Toppan Printing Co Ltd 透明導電性積層体の製造方法
WO2012157706A1 (fr) * 2011-05-17 2012-11-22 キヤノン電子株式会社 Filtre optique, dispositif optique, dispositif électronique et complexe antireflet
JP2015147952A (ja) * 2014-02-04 2015-08-20 コニカミノルタ株式会社 ガスバリア性フィルムの製造方法、ガスバリア性フィルム、電子デバイス、および、有機エレクトロルミネッセンス素子

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH111769A (ja) * 1997-06-10 1999-01-06 Canon Inc スパッタ膜の製造方法及びスパッタ膜
JP2003202405A (ja) * 2002-01-08 2003-07-18 Matsushita Electric Ind Co Ltd 反射防止膜を有する光学素子およびその製造方法
JP2008231532A (ja) * 2007-03-22 2008-10-02 Mitsubishi Materials Corp 被銅メッキ処理材の製造方法
JP2009196155A (ja) * 2008-02-20 2009-09-03 Dainippon Printing Co Ltd ガスバリアフィルム、ガスバリア膜の作製方法及び作製装置
JP2009220342A (ja) * 2008-03-14 2009-10-01 Oike Ind Co Ltd ガスバリアフィルムの製造方法及びガスバリアフィルム
WO2011077738A1 (fr) * 2009-12-25 2011-06-30 株式会社アルバック Film décoratif pour le moulage d'inserts, article formé par moulage d'inserts, procédé pour produire un film décoratif pour moulage d'inserts
JP2012061683A (ja) * 2010-09-15 2012-03-29 Toppan Printing Co Ltd 透明導電性積層体の製造方法
WO2012157706A1 (fr) * 2011-05-17 2012-11-22 キヤノン電子株式会社 Filtre optique, dispositif optique, dispositif électronique et complexe antireflet
JP2015147952A (ja) * 2014-02-04 2015-08-20 コニカミノルタ株式会社 ガスバリア性フィルムの製造方法、ガスバリア性フィルム、電子デバイス、および、有機エレクトロルミネッセンス素子

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113441377A (zh) * 2021-06-29 2021-09-28 辽宁分子流科技有限公司 一种纳米银丝电极薄膜的制备方法

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